Li
2 6 9 2
B O F , a New Acentric Fluorooxoborate
Table 3. Crystallographic data for Li
2
B
6
O
9
F
2
.
spectrometer QMS 422 (Balzers, Hudson, USA) at a heating rate of
–
1
10 K·min up to 1273 K.
Chemical formula
Temperature /K
Formula weight
Crystal system
Li
298
260.74
2
B
6
O
9
F
2
Ionic conductivity was measured from a compact pressed powder pel-
let with a diameter of 6 mm and a thickness of 1.1 mm. The sample
is placed in an argon floated quartz tube between ion blocking silver
electrodes. The measurement was performed with an Novocontrol Al-
pha A 4.2 Analyzer in combination with the ZG-4 interface in a 2-
wire arrangement from 1 Hz up to 5 MHz during continuous heating
monoclinic
Space group, Z
Lattice constants /Å
Cc, 4
a = 4.8211(12)
b = 16.149(4)
c = 10.057(3)
(from powder data)
β = 92.003(5) °
–1
[35]
at a rate of 0.5 K·min , controlled by WinDeta program.
The bulk
Volume /Å3
782.5(3)
[36]
conductivity was calculated by using the WinFit
program.
Density (calculated) /g·cm–3 ρ = 2.213
Crystal size /mm
Diffractometer
0.12 ϫ 0.10 ϫ 0.08
SMART APEX I (Bruker AXS
Karslsruhe)
Acknowledgement
X-ray radiation, λ /Å
Monochromator
α
Mo-K , 0.71073
graphite
0.23
The authors thank to Dr. H. Nuss for performing the single crystal
measurement.
Absorption coefficient μ /
–
1
mm
θ range /°
2.5–27.5
Index range
–6 Յ h Յ 6, –20 Յ k Յ 20, –13 Յ l
Յ 13
References
Independent reflections
Transmission tmin, tmax
No. of parameters
1748
0.6192, 0.7469
172
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631.
2
2
2
1
R [F Ͼ 2 σ (F )], wR(F ) 0.030, 0.076
Absolute structure param-
eter
0.4(6)
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Δρmin, Δρmax /e·Å–3
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Table 4. Atomic coordinates and equivalent isotropic displacement pa-
2
rameters Ueq /Å for Li
2
B
6
O
9
F
2
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Atom Site
x
y
z
U
eq
[
[
[
9] H. König, R. Hoppe, Z. Anorg. Allg. Chem. 1978, 439, 71.
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Li1
Li2
B1
B2
B3
B4
B5
B6
O1
O2
O3
O4
O5
O6
O7
O8
O9
F1
4a
4a
4a
4a
4a
4a
4a
4a
4a
4a
4a
4a
4a
4a
4a
4a
4a
4a
4a
0.1174(9)
–0.0365(2)
0.2424(2)
–0.1327(1)
–0.0338(1)
0.1469(1)
–0.2441(1)
0.1626(1)
0.0937(1)
–0.1182(1)
–0.0573(1)
0.0806(1)
–0.3046(1)
0.1641(1)
–0.1963(1)
–0.2307(19
0.1509(1)
0.0342(1)
0.0523(1)
0.1402(1)
0.8789(4)
1.0485(4)
0.9838(2)
1.1446(2)
0.7223(2)
0.8417(2)
1.2564(2)
1.0864(2)
0.8705(1)
1.0159(1)
0.7479(2)
0.8294(1)
0.5967(1)
0.9508(1)
0.7448(1)
1.1466(2)
1.1821(1)
0.9820(1)
1.0301(1)
0.0305(8)
0.0329(8)
0.0161(4)
0.0204(4)
0.0201(4)
0.0174(4)
0.0174(4)
0.0181(4)
0.0176(3)
0.0195(3)
0.0329(4)
0.0247(3)
0.0184(3)
0.0197(3)
0.0220(3)
0.0275(3)
0.0241(3)
0.0295(3)
0.0339(3)
–0.3047(9)
–0.3425(4)
–0.1368(5)
0.5990(5)
0.8459(4)
0.4646(4)
0.1190(5)
0.4612(3)
–0.1869(3)
0.7691(4)
1.0375(3)
0.5018(3)
0.8673(3)
0.6426(3)
0.3088(3)
0.0151(3)
0.2474(3)
–0.1023(3)
[
12] R. Bubnova, R. E. Dinnebier, S. Filatov, J. Anderson, Cryst. Res.
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91.
[
[
[
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[
[
[
[
F2
Further details on the structure determination may be obtained from
Fachinformationszentrum Karlsruhe, 76344 Eggenstein-Lepoldshafen,
Germany on quoting CSD number 423435.
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2
4, 785.
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1, 519.
–1
Infrared spectra (range: 400–4000 cm ) were recorded using the FT-
IR spectrometer IFS 113v (Bruker Optics, Karlsruhe, Germany)
equipped with vacuum optics and Grenzel interferometer. Sample pel-
lets (pre-dried KBr + sample, diameter 13 mm) were prepared in an
inert atmosphere glove box.
5
[
26] R. A. Nyquist, R. O. Kagel, Handbook of Infrared and Raman
Spectra of Inorganic Compounds and Organic Salts, Vol. 4, Aca-
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Thermal analysis was performed with the instrument STA 409 C [28] D. Chackraburtty, Acta Crystallogr. 1957, 10, 199.
Netzsch GmbH, Selb, Germany) connected with a quadrupole mass [29] M. J. Clark, H. Lynton, Can. J. Chem. 1969, 47, 2943.
4
(
Z. Anorg. Allg. Chem. 2011, 2148–2152
© 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim
www.zaac.wiley-vch.de
2151